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8 Performing a Measurement

D52IB001EN-G

45

2. Take out the heater insulation from the acces-

sory box delivered with the TTK 600 and place it
over the heater. See Fig. 9for further details.

3. Mount the heating block by reversing the actions

from point 1.

Fig. 49: Sample on standard sample holder

8.2.2 Additional Information for the Trans-
mission Sample Holder

The transmission sample holder (1) of TTK 600 is
made of nickel providing a good thermal conductivi-
ty and mechanical properties as well as high corro-
sion resistance.

A Pt100 sheath resistance temperature sensor (2) is
encapsulated in the sample holder (1), providing ex-
act temperature measurement. A connector for the

Pt100 (3) permits fast and easy exchange of the
sample holder. An additional convection heating is
provided by the connection of the gas hose (4) to the
gas connector on the right side of the instrument (5).
This additional heating mechanism ensure a minimi-
zation of the temperature deviation between dis-
played and real sample temperature. To protect the
detector, use the beamstop (6) at low 2

Θ

angles.

Fig. 50: Sample on transmission sample holder

8.2.3 Samples for the Capillary Sample
Holder

For information on preparing samples for the capil-
lary sample holder, refer to the instruction manual
Capillary Sample Holder for TTK 600.

NOTICE

Risk of damage.

Take care that the graphite foil that provides
improved thermal contact between sample
holder and heating/cooling block is in a good
condition (no visible scratches). Otherwise it is
strongly recommended to replace the graphite
foil with a new one in order to minimize the tem-
perature deviation between displayed and real
sample temperature.

1

2

3

NOTICE

Risk of damage.

Take care that the graphite foil that provides
improved thermal contact between sample
holder and heating/cooling block is in a good
condition (no visible scratches). Otherwise it is
strongly recommended to replace the graphite
foil with a new one in order to minimize the tem-
perature deviation between displayed and real
sample temperature.
Detailed information on the replacement of the
graphite foil are given in the service manual of
TTK 600.

1

2

3

4

5

6

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Summary of Contents for TTK 600

Page 1: ...Measure what is measurable and make measurable that which is not Galileo Galilei 1564 1642 Reference Guide TTK 600 Low Temperature Chamber with CCU 100 Control Unit ...

Page 2: ......

Page 3: ...is document or any part of it may not be reproduced changed copied or distributed by means of electronic systems in any form print photocopy microfilm or any other process without prior written permission by Anton Paar GmbH Trademarks registered trademarks trade names etc may be used in this document without being marked as such They are the property of their respective owner Further information P...

Page 4: ...Overheat Protection 19 2 6 Water Flow Controller 19 3 Checking the Supplied Parts 20 4 Installation 21 4 1 Installation Overview 21 4 2 Installation Requirements 22 4 2 1 X Ray Diffractometer Requirements 22 4 2 2 Electrical Requirements 23 4 2 3 Cooling Water Requirements 23 4 2 4 Requirements for Liquid Nitrogen Cooling 23 4 2 5 Requirements for Compressed air Cooling 23 4 2 6 Vacuum Equipment R...

Page 5: ...2 2 Additional Information for the Transmission Sample Holder 45 8 2 3 Samples for the Capillary Sample Holder 45 8 2 4 Taking out the Sample Holder 46 8 2 4 1 Standard Sample Holder 46 8 2 4 2 Transmission Sample Holder 46 8 2 4 3 Battery Sample Holder 47 8 2 5 Applying the Sample 48 8 2 5 1 Powder Samples for the Standard Sample Holder 48 8 2 5 2 Bulk Samples for the Standard Sample Holder 48 8 ...

Page 6: ...r Analysis 63 10 4 Technical Support 66 11 Maintenance 67 11 1 Routine Maintenance 67 11 2 Check the Functioning of the Flow Controller 67 11 3 Exchanging of Parts 67 11 3 1 Switching off the Instrument 67 11 3 2 Exchanging the Graphite Foil 67 11 3 3 Replacing the Window Foil 69 11 3 4 Replacing the O rings 69 11 4 Checking and Replacing Mains Fuses 70 Appendix A Technical Data 71 Appendix B Samp...

Page 7: ...ng any applicable operations In case of damage or malfunction do not con tinue operating TTK 600 Do not operate the instrument under conditions which could result in damage to goods and or injuries and loss of life Check TTK 600 for chemical resistance to the samples and cleaning agents Maintenance and service The results delivered by TTK 600 not only depend on the correct functioning of the instr...

Page 8: ...ded could result in death or serious injury CAUTION Description of risk Caution indicates a hazardous situation which if not avoided could result in minor or moderate injury NOTICE Description of risk Notice indicates a situation which if not avoided could result in damage to property CAUTION Hot surface This symbol calls attention to the fact that the respective surface can get very hot Do not to...

Page 9: ...hat the respective surface can get very hot Do not touch this surface without adequate protective measures 1 1 1 CAUTION Cold surface This symbol calls attention to the fact that the respective surface can get very cold Do not touch this surface without adequate protective measures Wear protective gloves Wear protective gloves when handling the TTK 600 Wear safety goggles Wear safety goggles when ...

Page 10: ...or the instrument With the liquid nitrogen cooling equip ment the temperature range is 190 C to 600 C With the compressed air cooling equipment the temperature range is 20 C to 600 C The sample can be cooled heated in vacuum or various gas at mospheres The sample temperature is controlled by a control unit CCU 100 This control unit is installed in spe cial compartments in the diffractometer or in ...

Page 11: ...e used type of sample holder 1 This is a nominal limit The true limit is the dew point temperature of the ambient air 2 Observe the pressure dew point requirements for the compressed air given in appendix A in order to avoid icing of the cryostat 3 Recommended heating rate slope for the battery sample holder transmission 20 C for the tem perature range CL cooling limit refer to chapter 6 3 1 The s...

Page 12: ...f X ray scans is re quired we recommend to use a motorized z align ment stage For TTK 600 the sample holder displacement during heating and cooling is approx 0 1 mm 2 3 2 Chamber Housing with Connectors Fig 5 Chamber housing with connectors 1 Blind plug for optional additional connections 2 Cooling water hose inlet 3 Cooling water hose outlet 4 Connection cable to CCU 100 5 Connector for sample co...

Page 13: ...ide the sample chamber 1 O ring seal 2 Knife edge 3 Guiding rods for beam stop 4 Beam Stop only for transmission configuration 5 Sample holder fixing ring 6 Graphite foil 7 Cryostat 8 Pt100 plug connector For detailed information on the materials used in the TTK 600 please refer to appendix A The temperature of the sample holder is controlled with a combination of resistance heater and cryo stat T...

Page 14: ...vironment can be used which inhibits the loss of heat to the surrounding atmosphere inside the TTK 600 The sample holder environment can be equipped with a graphite nickel or Kapton foil others on request To mount the sample holder environment see chap ter 8 4 2 Mounting the Standard Sample Holder Heating Environment Fig 9 Standard sample holder heating environment 1 Standard sample holder heating...

Page 15: ... steps can be found in chapter 8 4 5 The sample holder for the antechamber is different compared to the standard sample holder The most important difference is that this type of sample hold er has no integrated Pt100 temperature sensor If the antechamber for TTK 600 is used the tempera ture of the thermocouple inside the heater is used to measure the temperature For the recognition of this type of...

Page 16: ...ter 2 3 2 and controlled by CCU 100 CCU 100 automatically turns off the cooling when it is not needed to save liquid nitrogen compressed air 2 4 1 Liquid Nitrogen Cooling Equipment The LN2 cooling equipment consists of the following components Low Temperature Equipment for Venturi Nozzle cat no 164578 Liquid Nitrogen Container Dewar 60 L cat no 166462 or Liquid Nitrogen Container Dewar 100 L cat n...

Page 17: ...Venturi nozzle is provided by CCU 100 Active cooling is only needed to cool the sample holder to temperatures around room temperature and be low The so called Cooling Limit CL defines the threshold temperature for active cooling The value can be changed between 20 and 55 C see chapter 6 3 1 for further information If the tempera ture set point is CL CCU 100 opens the com pressed air connection to ...

Page 18: ...in parts of CCU 100 are the main board the micro controller for the temperature control and the power module The micro controller controls the sample holder temperature based on the measured temperature and the user defined target values The power module provides variable electrical power for the heater inside TTK 600 depending on the control signal from the micro controller 2 5 1 CCU 100 Front Pa...

Page 19: ...t no 164877 monitors the flow of cooling water through the housing of the sample chamber It is a water flow dependent switch which is connected to CCU 100 If there is not enough water flow CCU 100 switches to Standby heater off mode the Error LED on the front panel starts to flash and shows an alarm mes sage E03 In addition a thermoswitch is mounted on the sam ple chamber to protect the device fro...

Page 20: ... on label 159900 159930 1 1 1 2 1 and or 1 CCU 100 Combined Control Unit Mains cables Connection cable to TTK 600 sample chamber Mains fuses RS232 cable to control PC Low Power Module CCU 135000 176730 1 1 1 Flow Controller CCU Pressure regulator Water flow monitor 164877 1 1 1 with Liquid Nitrogen Cooling Equipment Low temperature equipment for Venturi nozzle Liquid nitrogen container Dewar 60L o...

Page 21: ...quirements following the schematic diagrams Fig 24 Installation diagram for TTK 600 with liquid nitrogen cooling equipment CCU 100 rear panel POWER RS 232 AIR OUT 1 AIR IN LAN Sensors Heater Heater Out 1 Out 2 Flow Sensor Low Power Module LN2 VESSEL LN2 Gas exhaust system TTK 600 SAMPLE CHAMBER L 5m L 3 5m Ø 4cm water out P water in DIFFRACTOMETER CABINET L 3 5m Ø 4cm 6 4 3 WATER FLOW MONITOR 2 ba...

Page 22: ...niometer is possible but during low temperature operation the LN2 hoses get stiff and rotatability of the sample chamber may be limited Clearance around goniometer axis at least 125 mm see also appendix A Feedthroughs for two LN2 hoses with 40 mm each two water hoses with 4x6 mm two electri cal cables with 5 mm and a vacuum hose with CCU 100 rear panel POWER RS 232 AIR OUT 1 AIR IN LAN Sensors Hea...

Page 23: ... rel TIP Anton Paar GmbH offers suitable Dewars with 60 L and 100 L volume see appendix B 4 2 5 Requirements for Compressed air Cooling Pressure 6 to 8 bar rel Flow rate 120 l min at 7 bar pressure dew point 7 bar for operating temperature 5 C 25 C for operating temperature 5 C 10 C Purity acc DIN 8573 1 solid particle class 3 or better oil class 2 or better Connector of air supply 5 pneumatic cou...

Page 24: ... part Make sure that the alignment screw 1B is sur rounded by the two parts 1A Adapter for Battery Sample Holders When changing from standard sample holders to the battery sample holders ensure that the guiding pins of the TTK 600 are aligned in the correct posi tion on the adapter There are different positions for standard sample holders the reflection battery sam ple holder and the transmission ...

Page 25: ... connector Sensors Heater see Fig 21 10 Make sure the mains switch on CCU 100 is OFF and connect the mains power cable to the POWER connector see appendix 21 1 4 6 Connecting CCU 100 with a Com puter The RS 232 serial port at the rear panel of CCU 100 allows you to connect the CCU 100 to a computer for remote control see Fig 21 4 A null modem RS 232 cable is required to connect the CCU 100 to a PC...

Page 26: ...e couplings tightly seal the hoses Neverthe less we recommend to turn off the water supply if you don t use TTK 600 for a longer period of time 4 8 Installing the Liquid Nitrogen Equipment Install the liquid nitrogen LN2 cooling equipment as follows 1 Feed the LN2 supply hoses through a suitable port in the diffractometer cabinet so that the LN2 connector is inside the cabinet see Fig 15 2 Place t...

Page 27: ... to the TTK 600 sample chamber proceed as fol lows Fig 30 Low Temperature Equipment 1 Insert the nozzle A of the LN2 connector B into the cooling device connector C on the sample chamber 2 Rotate the LN2 connector B with a gentle push upwards until it fully slides into the cooling device connector C 3 Turn the LN2 connector B counter clockwise so that it is parallel to the goniometer to lock it on...

Page 28: ...vice unit B This can be done either directly or with the short hose C supplied with the instrument 3 Connect the Air Service Unit to the compressed air supply of the laboratory 4 Connect the male connector of the pneumatic hose to the outlet of the air service unit or the compressed air dryer respectively 5 Set the pressure on the Air Service Unit to 7 bar TIP 7 bar is the standard value The press...

Page 29: ... Nitrogen switch the cooling mode switching valve to the corresponding position and install the air cooling equipment Fig 31 or the Low Temperature Equipment Fig 30 to the chamber 5 on Fig 5 4 11 Mounting the Gas Vacuum Con nector The gas vacuum connector allows to supply and ex tract gas from the TTK 600 and to apply vacuum to the chamber The gas vacuum connector is mount ed to the lid of the TTK...

Page 30: ...g 35 Anton Paar GmbH standard vacuum equipment TIP Make sure that both the housing s sealing sur face and the O ring of the lid are clean and slightly coated with vacuum grease If oxygen free sample environment is needed con nect the vacuum system to the gas vacuum connec tor instead of the blind plug Between the gas vacuum connector and the cross piece a valve MUST be used to protect the vacuum g...

Page 31: ...en using a Kapton foil For installation of the convection heater proceed as follows 1 Dismount the blind cover on the right side of the housing unscrew the two screws NOTICE The corner valve is not included in the vacuum equipment but can be ordered as an accessory refer to appendix D To protect the vacuum equipment from pressure a valve MUST be installed between gas vacuum connector and the vacuu...

Page 32: ... 4 13 Mounting the Electrode Connector and the Connector Box For the use of the battery sample holder it is neces sary to mount the electrode connector and the con nector box to TTK 600 in order to be able to put an electrical load on the battery materials under inves tigation For the installation of these parts proceed as fol lows 1 Dismount the blind cover on the right side of the housing unscre...

Page 33: ...nnector 3 Connect the plug of the connector box to the electrode connector on TTK 600 Fig 39 Connector box for battery sample holder The connector box has two banana type connectors for the connection of an external electrical measur ing device 1 ...

Page 34: ...he X ray beam Θ zero line Perform the alignment of TTK 600 at room tempera ture Alignment is best done in two steps 1 Coarse alignment with the upper edge of the empty sample holder 2 Fine alignment with the alignment slit in the alignment block 5 1 1 Height Alignment with Rigid Adapter The height z position of the sample chamber rela tive to the X ray beam can be adjusted with the alignment equip...

Page 35: ...e a narrow X ray beam small beam height and select a detector area which is larger than the beam 3 Set the goniometer to Θ 0 2Θ 0 4 Move the chamber to the Θ zero line as follows If you have mounted the standard sample holder Lower the chamber until no parts are in the X ray beam path and determine the maximum beam intensity Imax Lift the chamber until the X ray beam is com pletely blocked and det...

Page 36: ...d limits depending on your experimental needs 5 4 Checking the Instrument Condition Before you start operation Make sure that TTK 600 is installed correctly and that no collisions between the sample chamber and components of the diffractometer can occur Make sure that the cooling water hoses con nected to the inlet outlet nozzles are protected against unintentional disconnection Check whether all ...

Page 37: ... flashing the display shows E03 to indicate that there is no water flow 2 Turn on the cooling water supply The alarm message disappears and the flashing of the Error LED stops 3 Check whether the correct Cooling Type param eter is set as described in chapter 6 3 LN2 for liquid nitrogen cooling CAir for compressed air cooling 4 Press the HEATER button to start control of the sample holder temperatu...

Page 38: ...00 is not possible on the controller itself However the deliv ered software for the controller allows to program a temperature profile see the corresponding software manual that was delivered with the instrument 6 1 Front Panel of the Instrument The front panel of CCU 100 contains the keypad the status LEDs and the display which are described in the following section Fig 42 Front panel of CCU 100 ...

Page 39: ...n the right side of the display see chapter 6 2 1 different informa tion In the normal operation mode process value LED is green the display shows the actual tem perature of the sample holder of TTK 600 By pressing the SCROLL button the set point LED is green which means that the target set point tem perature can now be changed by using the UP or DOWN button By pressing the SCROLL button twice the...

Page 40: ... be changed in the config mode are described in the following table Parameter Description Note rAte Heating Cool ing Rate value C min Default value 20 C min cOn cOFF Allows to switch the cooling of the instrument on and off Ln2 CAir noC Toggle between the CCU 100 configurations for LN2 cooling compressed air cooling and no cooling CL Temperature below which cooling is per manently acti vated Value...

Page 41: ...ot activated until the sample temperature reaches 300 C Going below this limit the CCU 100 auto matically switches on the used cooling equipment 6 5 1 Controlling the Liquid Nitrogen Cooling LN2 cooling is turned ON if the temperature set point is below the Cooling Limit CL The COOLING LED see chapter 6 2 1 indicates that CCU 100 supplies liquid nitrogen to the sample chamber and that the LN2 cool...

Page 42: ...00 Proceed as follows to heat or cool the sample to the desired tempera ture 1 Make sure that the heater is switched on 2 Set the desired heating cooling rate on the parameter page of CCU 100 See chapter 6 3 1 3 Push the scroll button one time SP LED green and set the desired target temperature by using the UP DOWN buttons 4 Wait until the displayed sample holder tempera ture has reached the targe...

Page 43: ... 1 LN2 Consumption and Operating Time The typical consumption of LN2 does not exceed 4 L h This corresponds to a measuring time of max 25 hours in case that a Dewar vessel with a volume of 100 L is used 7 2 Typical Cooling Curves For typical sample holder cooling curves with maxi mum cooling rate for the liquid nitrogen cooling equipment and the compressed air cooling equip ment refer to chapter 8...

Page 44: ... Sample 8 2 1 Additional Information for the Standard Sample Holder The sample holder 1 of the TTK 600 is made of nickel providing a good thermal conductivity and mechanical properties as well as high corrosion re sistance Three sample holders with different depths of the sample cavity 0 8 mm 0 2 mm or flat are avail able In addition a zero background holder with a specially cut silicon insert can...

Page 45: ...n dis played and real sample temperature To protect the detector use the beamstop 6 at low 2Θ angles Fig 50 Sample on transmission sample holder 8 2 3 Samples for the Capillary Sample Holder For information on preparing samples for the capil lary sample holder refer to the instruction manual Capillary Sample Holder for TTK 600 NOTICE Risk of damage Take care that the graphite foil that provides im...

Page 46: ...ching off the heater there can be dangerously hot or cold sur faces inside the sample chamber Always check on the display of CCU 100 that the sample holder temperature is below 50 C before you open the sample chamber and touch any parts inside If CCU 100 shows an error message use a suit able temperature sensor to measure the actual temperature of the parts inside the sample chamber Always switch ...

Page 47: ...sor right side while lifting the cable of the temperature sensor over the heat ing block left side 8 2 4 3 Battery Sample Holder In order to remove the sample from the TTK 600 proceed as follows 1 Switch off the heater of the CCU 100 2 Open the lid 3 Disconnect the electrode connector from the TTK 600 housing 4 Disconnect the Pt100 connector 5 Unscrew the fixing screw of the sample holder with the...

Page 48: ...th of 0 2 mm and a flat sample holder are also available The alignment stage allows you to compensate for the difference in height between the sample holder and sample holder groove 8 2 5 3 Powders and Pastes for the Transmission Sample Holder The procedure for preparing powder and paste samples for the transmission sample holder is de scribed below 1 Place the delivered mounting tool on a flat su...

Page 49: ...r the first clamping piece 5 Add the distance piece to the stack Different distance pieces are available 1 mm 0 5 mm and 0 25 mm 6 Fill the central room in the distance piece with your sample Powders and pastes can be used Use a spatula to compress the sample within the compartment 7 Add the second foil to the stack 8 Add the clamping piece 9 Fix the stack with the two screws ...

Page 50: ...e coin cell 6 Place first the Kapton foil 3 on the cathode fol lowed by the graphite foil 2 The use of the graphite foil is optional See also chapter 8 3 4 7 Mount the lid 1 of the battery sample holder again by the use of the 4 Torx screws An exploded view drawing showing all the compo nents including the assembled coin cell is shown below Fig 52 Exploded view drawing of the battery sample holder...

Page 51: ...tions and foil materials The following guideline can be used for the optimal choice of the foil material for the transmission sam ple holder 8 3 1 Temperature Range Whenever the Kapton foil is used the max tem perature of the experiment must not exceed 230 C Higher temperatures would result in a destruction of the foil material Both nickel and graphite do not limit the tempera ture range of the ex...

Page 52: ...ensure the smallest possible difference between the temperature on the CCU 100 and the actual sample temperature The graphite foils must be used in combination with the Kapton foils to ensure the gas tightness of the sam ple holder The absolute temperature differences for the differ ent foil combinations on the reflection and transmis sion holders in a nitrogen atmosphere are shown below Fig 55 Di...

Page 53: ...ounting the Standard Sample Holder Heating Environment To mount the sample holder environment proceed as follows 1 Remove the sample holder 2 Remove the cooling equipment from the instru ment 3 Demount the heating cooling block of the instru ment from the housing by unscrewing the knurled screws as shown in the following pic ture Take care to hold the heating block while unscrewing the last screw ...

Page 54: ...ogram Background measure ments for Nickel and Graphite can be found in chapter 8 3 To replace the foil of the sample holder heating en vironment and to demount mount the antiscatter shield for the sample holder heating environment proceed as follows 1 Unscrew the two screws of the foil clamps and take of the clamps and the foil 2 Mount demount the antiscatter shield 3 Replace the foil and ensure t...

Page 55: ...ector of the gas con nector to the delivered gas hose of the instru ment 8 Connect the other end of the gas hose to the gas reservoir 9 The optimal flow that is needed depends on the choice of the foils Further information can be found in chapter 8 3 Guideline for the correct choice of conditions and foil materials Fig 57 Transmission Sample Holder 1 Sample holder fixing ring 2 Pt100 3 Fixing scre...

Page 56: ...le holder loader 4 Gas tight compartment 5 Vacuum flange 6 Torx screw for sample holder fixation 7 Mounting screws 1 Place the antechamber as depicted in Fig 58 A in the glove box In order to do so a separate mount is contained in the delivery of the ante chamber see appendix 12 2 Fill the sample into the sample holder 1 3 Pull back the sample loader 3 4 Close the gas tight compartment 4 by pushin...

Page 57: ...box if neces sary 8 4 6 Mounting and Use of the Battery Sam ple Holders Before mounting the battery sample holder ensure that the chamber is mounted on the adapter in the correct position for the sample holder which will be used Details for the mounting of the adapter can be found in chapter 4 3 Battery Sample Holder Reflection Fig 59 Reflection sample holder To mount the battery sample holder ref...

Page 58: ...rements for the operation with air inside the chamber Leave the vacuum flange open to allow release of gas during heating in order to avoid overpressure in side the chamber 8 5 2 Operation under Vacuum TTK 600 can be evacuated to approx 1x10 2 mbar with a rotary pump 4 2 m3 h In case that high vacuum is needed TTK 600 can also be evacuated to approx 1x10 4 mbar using a turbomolecular pump Experime...

Page 59: ...uipment from pressure a ball valve MUST be installed between gas vac uum connector and the vacuum equipment BEFORE opening the gas inlet and applying pressure the ball valve has to be closed as dam age of the vacuum parts will occur Vent the chamber slowly to avoid the sample being detached from the sample holder Detailed information about the set up for opera tion with vacuum are given in the ins...

Page 60: ... room temperature 2 Turn off the heater and remove the sample holder 3 Prepare the sample and insert the sample holder with the sample 4 Close the lid 5 Turn on the heater 6 If necessary align the sample height at 25 C before starting an experiment This can be done by measuring the peak position of a known phase in the sample and re adjusting the sam ple chamber height until the peak is at the cor...

Page 61: ...transformation or thermal lattice expansion Lists of reference materials with thermal data and instructions for doing validation measurements can be found in the XRD literature TIP Try to avoid measurements in vacuum be cause temperature deviation in vacuum is much larger than if the chamber is filled with gas When ever possible use dry nitrogen or helium gas in stead of vacuum 8 8 2 Effective Hea...

Page 62: ...on in the Dewar again 6 Start the next experiment TIP The above mentioned procedures prevent con densation of moisture inside the liquid nitrogen cool ing equipment 7 When using the compressed air cooling equip ment III Turn off the compressed air supply 1 Turn off the cooling water 2 Turn off CCU 100 completely In order to remove TTK 600 from the diffractometer continue as follows 1 Completely tu...

Page 63: ... current cable E09 CCU 100 Air Cool ing Fail The protective thermoswitch inside CCU 100 is activated E10 Other Messages Internal errors of CCU 100 contact Anton Paar GmbH E11 Sensor Spread Failure Activated in case of too big temperature difference between the sensors sample holder and heater E12 Flow Con trol Exten sion missing Activated in case of missing flow control ler E13 Power Stage Fault C...

Page 64: ...e and connectors cause action water hoses dis connected Connect the water hoses on TTK 600 to the cooling water circuit no cooling water Turn on the cooling water flow controller disconnected Connect the water flow con troller to the CCU 100 insufficient cool ing water supply Make sure the water pres sure is between 2 3 bar and the flow rate is 0 7 1 5 l min flow controller does not switch Contact...

Page 65: ...ature After that heat the sample holder of TTK 600 to 200 C for one hour and blow dry air or nitrogen through the cryo stat by removing the plug and inserting a suitable gas hose in the inlet connection NOTICE Risk of damage The pressure of the drying gas dry air or nitro gen must not exceed 0 4 bar during the drying of the cryostat Higher pressures could damage the heater of the instrument cause ...

Page 66: ...ar Strasse 20 A 8054 Graz AUSTRIA Europe Tel 43 316 257 0 Fax 43 316 257 257 E mail info anton paar com Web www anton paar com cause action Low Power mod ule not installed correctly Make sure the Low Power module seats correctly no gap on the side or inserted crookedly If not contact your diffrac tometer manufacturer or Anton Paar GmbH Low Power mod ule not installed Check if the Low Power module ...

Page 67: ...e instrument Perform the recommended maintenance work regu larly to ensure the smooth long term operation of the instrument 11 3 2 Exchanging the Graphite Foil The graphite foil between the sample holder and the heating cooling block ensures good heat transfer from the heater to the sample holder Therefore it is essential to regularly check the condition of the graphite foil It is recommended to e...

Page 68: ...e 5 Remove the sample holder fixing ring by unscrewing the two screws with the supplied Torx driver 6 Remove the sample holder fixation ring and the old graphite foil 7 Replace the old graphite foil with a new one by placing it centrically over the heater Mount the instrument by reversing the above men tioned steps ...

Page 69: ...nt it again in the groove 6 Place the window foil over the nipples that hold the foil in place Make sure the holes for the screws in the foil are in the correct places over the holes for the screws of the chamber 7 Place the clamping pieces back on the chamber 8 Tighten the 20 screws beginning with the upper most four 11 3 4 Replacing the O rings Commercially available O rings made of Viton are us...

Page 70: ...Check the fuse or exchange the defective fuse The two mains fuses are made of ceramic Spec 2 x T 6 3 A 5 Put the fuse box back into the cavity of the power supply WARNING High voltage Make sure that BEFORE performing any ser vice maintenance work of the CCU 100 the instrument is disconnected from the mains sup ply Only use the specified fuse types NOTICE Risk of damage Service and or maintenance p...

Page 71: ...es air inert gas N2 vacuum 10 4 mbar Pressure max 2 bar relative Control unit CCU 100 Temperature sensor1 TC Type K Temperature sensor2 Pt100 Temperature accuracy1 2 C Heating method Resistance heater Cooling methods compressed air cooling or liquid nitrogen cooling Compressed air consumption 6 bar 120 l min Liquid nitrogen consumption max 4 l h 1 Sample holder temperature values depending on oper...

Page 72: ...50 x 410 x 180 mm Weight approx 13 kg Voltage mains AC 100 240 V Frequency mains 50 60 Hz Power consumption max 250 VA Mains fuses 2 x T 6 3A H 5x20 mm ceramic tube Overvoltage category II according to EN 61010 1 Voltage output DC 48 V Current output max DC 4 A Heater fuse 2 x T4 A SMD Flow rate 0 7 to 1 5 l min Temperature 15 to 25 C Pressure 2 to 8 bar Pressure 6 8 bar rel Flow rate 120 l min at...

Page 73: ...elf evaporation rate 0 2 L d Opening dimension DN 50 KF Ambient temperature 5 35 C Ambient humidity 80 max not condensing Maximum operating altitude 3000 m above sea level Pollution degree 2 according to EN 61010 1 TTK 600 is for INDOOR USE ONLY Protect the instruments from moisture ...

Page 74: ...Appendix B Sample Chamber Dimensions 74 D52IB001EN G Appendix B Sample Chamber Dimensions ...

Page 75: ...Appendix C Declaration of Conformity D52IB001EN G 75 Appendix C Declaration of Conformity ...

Page 76: ...ARD SAMPLE HOLDER WITH Pt100 0 8mm DEPTH 162262 STANDARD SAMPLE HOLDER TTK 600 WITH Pt100 0 2mm DEPTH 162263 STANDARD SAMPLE HOLDER TTK 600 WITH Pt100 FLAT 163290 CAPILLARY SAMPLE HOLDER TTK 600 164863 TRANSMISSION SAMPLE HOLDER TTK 600 25420 ZERO BACKGROUND INSERT TTK 164864 SET OF GRAPHITE FOILS TTK 600 10 PCS 70175 VACUUM GREASE 20g 164865 SET OF KAPTON FOILS 5 pcs 164866 SET OF O RINGS 8415 FI...

Page 77: ...Appendix D Spare Parts and Accessories D52IB001EN G 77 176383 COOLING MODE SWITCHING VALVE ...

Page 78: ...INFORMATION ON INGREDIENTS CHEMICAL NAME CAS mole EXPOSURE LIMITS IN AIR ACGIH TLV OSHA PEL NIOSH OTHER TWA STEL TWA STEL IDLH ppm ppm ppm ppm ppm ppm Nitrogen 7727 37 9 99 99 There are no specific exposure limits for Nitrogen Nitrogen is a simple asphyxiant SA Oxygen levels should be maintained above 19 5 Maximum Impurities 0 01 None of the trace impurities in Liquid Nitrogen contribute significa...

Page 79: ...th rapidly expanding gas poses a frostbite hazard OTHER POTENTIAL HEALTH EFFECTS Contact with cryogenic liquid or rapidly expanding gases which are released under high pressure may cause frostbite Symptoms of frostbite include change in skin color to white or grayish yellow The pain after contact with liquid can quickly subside HEALTH EFFECTS OR RISKS FROM EXPOSURE An Explanation in Lay Terms Over...

Page 80: ...rmore the relatively warm water greatly increases the evaporation rate of Nitrogen If large concentrations of Nitrogen gas are present the water vapor in the surrounding air will condense creating a dense fog that may make it difficult to find fire exits or equipment Liquid Nitrogen when exposed to the atmosphere will produce a cloud of ice fog in the air upon its release UNUSUAL FIRE AND EXPLOSIO...

Page 81: ...e Use designated CGA fittings and other support equipment Do not use adapters Do not use oils or grease on valve fittings or equipment Leak check system with leak detection solution Immediately contact the supplier if there are any difficulties associated with operating container valve After Use Close main container valve Mark empty container EMPTY NOTE Use only DOT or ASME code containers designe...

Page 82: ...re of magnesium powder and Liquid Nitrogen reacts very violently when lit with a fuse forming magnesium nitride Liquid Nitrogen is not corrosive to metals but the extreme cold can make some metals brittle HAZARDOUS POLYMERIZATION Will not occur CONDITIONS TO AVOID Contact with incompatible materials Cryogenic containers exposed to high temperatures or direct flame can rupture or burst 11 TOXICOLOG...

Page 83: ...ON Cryogenic containers should be transported in a secure position in a well ventilated vehicle The transportation of compressed gas cryogenic containers in automobiles or in closed body vehicles present serious safety hazards and should be discouraged NOTE Shipment of compressed gas cryogenic containers which have not been filled with the owners consent is a violation of Federal law 49 CFR Part 1...

Page 84: ... PROTECTION ACT CEPA PRIORITY SUBSTANCES LISTS Liquid Nitrogen is not on the CEPA Priorities Substances Lists WHMIS CLASSIFICATION Liquid Nitrogen is categorized as a Controlled Product Hazard Class A as per the Controlled Product Regulations OTHER CANADIAN REGULATIONS Not applicable 16 OTHER INFORMATION MIXTURES When two or more gases or liquefied gases are mixed their hazardous properties may co...

Page 85: ...Appendix F Warranty D52IB001EN G 85 Appendix F Warranty The warranty regulations for TTK 600 are in accordance with the General Terms of Delivery of the Austrian Electrical and Electronic Industry ...

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